CN107117753A - A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized - Google Patents
A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized Download PDFInfo
- Publication number
- CN107117753A CN107117753A CN201610102540.XA CN201610102540A CN107117753A CN 107117753 A CN107117753 A CN 107117753A CN 201610102540 A CN201610102540 A CN 201610102540A CN 107117753 A CN107117753 A CN 107117753A
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- Prior art keywords
- wool
- sodium
- making herbs
- solar cell
- utilized
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
- C01B21/46—Purification; Separation ; Stabilisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
- C01B7/196—Separation; Purification by distillation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized, comprising except processes such as fluosilicic acid, HF/HNO3 separation, purifying, the single chemicals or mixed chemical product of chemical stock solution grade used in process for etching are can obtain, the discharge of useless chemicals is substantially reduced.
Description
Technical field
The invention belongs to chemical waste fluid recycling field, especially relate to a kind of silicon solar cell making herbs into wool waste liquid and return
Receive the method utilized.
Background technology
The making herbs into wool process of silicon solar cell is that silicon face is carried out into prerinse and corrodes into class with highly basic or strong acid
Like the process of pyramid shape or alveolate texture.Chemicals used in alkali making herbs into wool is mainly sodium hydroxide or hydroxide
Potassium, isopropanol or ethanol, sodium metasilicate or matte additive；Chemicals used in sour making herbs into wool is mainly nitric acid, hydrogen
Fluoric acid.Process for etching includes the steps such as making herbs into wool, pickling, alkali cleaning, drying, the waste water and waste liquid that production process is produced
Mainly by acidic and alkaline waste water, hydrofluoric acid wastewater, organic wastewater.The present invention be directed to the production of the making herbs into wool process of polysilicon chip
The method that raw waste liquid is recycled.
Polycrystalline silicon texturing process produce waste liquid based on hydrofluoric acid wastewater, in waste liquid containing HF, HNO3,
Several key components such as H2SiF6 and micro metal ion.Conventional fluoride wastewater treatment technique is main at present
There are absorption method and the precipitation method.Absorption method is only applicable to low concentration fluoride waste.The precipitation method are applied in defluorinating process
Most extensively, it is suitable for handling high-concentration fluorine-containing waste water.Traditional treatment method is neutralized using Ca (OH) 2
Reaction, is generated the calcirm-fluoride of indissoluble, is removed with solid-liquid separation means from waste water.But solid waste CaF2 is brought,
New pollution is caused, and saturation solubilities of the CaF2 in water is 16.5mg/L, it is impossible to reach national waste water row
Put standard 10mg/L.
The content of the invention
For defect present in above prior art, the invention provides a kind of silicon solar cell making herbs into wool waste liquid
The method of recycling, comprising except processes such as fluosilicic acid, HF/HNO3 separation, purifying, can obtain process for etching
The single chemicals or mixed chemical product of chemical stock solution grade used, substantially reduce the discharge of useless chemicals.
Therefore, the technical solution adopted in the present invention is：What a kind of silicon solar cell making herbs into wool devil liquor recovery was utilized
Method, comprises the following steps：
The first step：Except fluosilicic acid process, i.e., sylvite or sodium salt are put into the reactive tank equipped with the making herbs into wool waste liquid
In, the waste liquid is 1 with the weight ratio for adding sylvite or sodium salt:1~1:Under 1.5,10 DEG C~30 DEG C temperature ranges
Reacted, material is fully contacted by way of stirring or being circulated with pump and reacted, then passed through
The mode of filtering or centrifugation carries out separation of solid and liquid；
Second step：Purification procedures, the purification procedures are the processes for being purified the waste liquid after above-mentioned processing,
Metal impurities ion is removed by way of rectifying.
Further, step is also included after the step one：
HF/HNO3 separation circuits；The HF/HNO3 separation circuits are 10%~50% salt for adding liquid quality,
Break azeotropic system, carry out rectifying and obtain single HF and HNO3.
Further, the sylvite or sodium salt added in the step one is potassium nitrate/sodium, potassium chloride/sodium, fluorination
One of which soluble-salt in potassium/sodium, potassium/sodium.
Further, the sylvite or sodium salt added in the step one is in solid potassium fluosilicate or prodan
One of which solid salt.
The beneficial effects of the invention are as follows：The inventive method is compared with other techniques, in the same of reduction discharging of waste liquid
When, supplemented with the fresh consumption of former chemicals, reduce the cost used.
Embodiment
Following embodiments describe the present invention in detail, but do not limit the scope of the invention.But the protection model of the present invention
Enclose and be not intended to be limited to following examples.Person of an ordinary skill in the technical field is according to disclosed by the invention
Content, can be achieved the purpose of the present invention.
Embodiment 1
A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized, comprises the following steps：
The first step：Except fluosilicic acid process, i.e., sylvite or sodium salt are put into the reactive tank equipped with the making herbs into wool waste liquid
In, the waste liquid is 1 with the weight ratio for adding sylvite or sodium salt:1~1:Under 1.5,10 DEG C~30 DEG C temperature ranges
Reacted, material is fully contacted by way of stirring or being circulated with pump and reacted, then passed through
The mode of filtering or centrifugation carries out separation of solid and liquid；
Second step：Purification procedures, the purification procedures are the processes for being purified the waste liquid after above-mentioned processing,
Metal impurities ion is removed by way of rectifying.
As another improvement of technical solution of the present invention, also include step after the step one：
HF/HNO3 separation circuits；The HF/HNO3 separation circuits are 10%~50% salt for adding liquid quality,
Break azeotropic system, carry out rectifying and obtain single HF and HNO3.
As another improvement of technical solution of the present invention, the sylvite or sodium salt added in the step one is nitric acid
One of which soluble-salt in potassium/sodium, potassium chloride/sodium, potassium fluoride/sodium, potassium/sodium.
As another improvement of technical solution of the present invention, the sylvite or sodium salt added in the step one is solid
One of which solid salt in potassium fluosilicate or prodan.
Specifically, it is described except fluosilicic acid process is the fluosilicic acid using sylvite or sodium salt and fluosilicic acid formation indissoluble
Potassium or prodan, sylvite or sodium salt are put into the reactive tank equipped with mixed acid waste liquor, and fluosilicic acid is with adding potassium
The stoichiometric proportion of salt or sodium salt is 1:1~1:Reacted under 1.5,10 DEG C~30 DEG C temperature ranges, by stirring
Mix or the mode that is circulated with pump make material fully contact to be reacted, then filter or centrifugation by way of
Carry out separation of solid and liquid, the sylvite or sodium salt of addition are potassium nitrate (sodium), potassium chloride (sodium), potassium fluoride (sodium),
The soluble-salts such as potassium sulfate (sodium), solid potassium fluosilicate or prodan can be used as other chemicals raw material.
The HF/HNO3 separation circuits are the boiling point difference using HF and HNO3, pass through salt distillation or decompression
The mode of rectifying obtains single HF and HNO3.10%~50% salt of liquid quality in rectifying column is added, is beaten
Broken azeotropic system, carries out rectifying, and can suitably depressurize, and reduces boiling point.The process can be determined according to the actual requirements
Whether must carry out.HF/HNO3 nitration mixture is obtained if necessary to reclaim, then may skip this step be directly entered it is pure
Chemical industry sequence.
Purification procedures are the processes for being purified the waste liquid after above-mentioned processing, and metal is removed by way of rectifying
Foreign ion, carrying out purifying makes chemicals reach photovoltaic grade, so that making herbs into wool of the reusable edible to solar cell
In technique or other techniques.
The inventive method is compared with other techniques, while discharging of waste liquid is reduced, supplemented with former chemicals
Fresh consumption, reduce the cost that uses.
Claims (4)
1. a kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized, it is characterised in that comprise the following steps：
The first step：Except fluosilicic acid process, i.e., sylvite or sodium salt are put into the reactive tank equipped with the making herbs into wool waste liquid,
The waste liquid is 1 with the weight ratio for adding sylvite or sodium salt:1~1:Carried out under 1.5,10 DEG C~30 DEG C temperature ranges
React, material is fully contacted by way of stirring or being circulated with pump and reacted, then pass through filtering
Or the mode of centrifugation carries out separation of solid and liquid；
Second step：Purification procedures, the purification procedures are the processes for being purified the waste liquid after above-mentioned processing, are passed through
The mode of rectifying removes metal impurities ion.
2. a kind of method that a kind of silicon solar cell making herbs into wool devil liquor recovery as claimed in claim 1 is utilized, it is special
Levy and be：Also include step after the step one：
HF/HNO3 separation circuits；The HF/HNO3 separation circuits are 10%~50% salt for adding liquid quality, are beaten
Broken azeotropic system, carries out rectifying and obtains single HF and HNO3.
3. a kind of method that a kind of silicon solar cell making herbs into wool devil liquor recovery as claimed in claim 1 is utilized, it is special
Levy and be：The sylvite or sodium salt added in the step one be potassium nitrate/sodium, potassium chloride/sodium, potassium fluoride/sodium,
One of which soluble-salt in potassium/sodium.
4. a kind of method that a kind of silicon solar cell making herbs into wool devil liquor recovery as claimed in claim 1 is utilized, it is special
Levy and be：The sylvite or sodium salt added in the step one is wherein one in solid potassium fluosilicate or prodan
Plant solid salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610102540.XA CN107117753A (en) | 2016-02-24 | 2016-02-24 | A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610102540.XA CN107117753A (en) | 2016-02-24 | 2016-02-24 | A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized |
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| CN107117753A true CN107117753A (en) | 2017-09-01 |
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| CN201610102540.XA Pending CN107117753A (en) | 2016-02-24 | 2016-02-24 | A kind of method that silicon solar cell making herbs into wool devil liquor recovery is utilized |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640349A (en) * | 2018-05-25 | 2018-10-12 | 南京八度阳光太阳能科技有限公司 | A kind of silicon solar cell making herbs into wool waste collecting device |
| CN108716020A (en) * | 2018-05-29 | 2018-10-30 | 南京八度阳光太阳能科技有限公司 | A kind of making herbs into wool waste material recycling device used for solar batteries |
| CN110844885A (en) * | 2019-09-06 | 2020-02-28 | 浙江东氟塑料科技有限公司 | Method for recovering and regenerating hydrofluoric acid from waste liquid |
| CN111573640A (en) * | 2020-04-29 | 2020-08-25 | 南京理工大学 | Method and system for producing high-purity nitric acid by recovering fluorine-containing dilute nitric acid waste liquid |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5346557A (en) * | 1991-10-29 | 1994-09-13 | Hi-Silicon, Co., Ltd. | Process for cleaning silicon mass and the recovery of nitric acid |
| JP2007254254A (en) * | 2006-03-27 | 2007-10-04 | Hideki Yamamoto | Method for recovering mixed acid with increased compositional ratio of hydrofluoric acid from waste mixed acid liquid containing hydrofluoric acid |
| US20080053815A1 (en) * | 2006-08-31 | 2008-03-06 | Wacker Chemie Ag | Method for processing an etching mixture which is formed during the production of highly pure silicon |
| CN102745837A (en) * | 2012-07-18 | 2012-10-24 | 上海交通大学 | Method for treating and recycling glass thinning and etching waste liquor |
| CN103086555A (en) * | 2011-10-31 | 2013-05-08 | 库特勒自动化***(苏州)有限公司 | Treatment system and treatment method for silicon wafer etching waste water |
| CN103213991A (en) * | 2013-04-28 | 2013-07-24 | 苏州晶瑞化学有限公司 | Recovery and cyclic utilization technology for electronic-level waste acid mixture |
| JP2013163168A (en) * | 2012-02-13 | 2013-08-22 | Kurita Water Ind Ltd | Apparatus and method for refining fluoro-nitric acid waste solution |
| CN104986771A (en) * | 2015-07-02 | 2015-10-21 | 苏州晶洲装备科技有限公司 | Treatment method for multi-crystalline silicon texturization etching waste liquid |
| CN204981156U (en) * | 2015-07-02 | 2016-01-20 | 苏州晶洲装备科技有限公司 | Recovery system of recycling of polycrystalline silicon making herbs into wool sculpture waste liquid |
-
2016
- 2016-02-24 CN CN201610102540.XA patent/CN107117753A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5346557A (en) * | 1991-10-29 | 1994-09-13 | Hi-Silicon, Co., Ltd. | Process for cleaning silicon mass and the recovery of nitric acid |
| JP2007254254A (en) * | 2006-03-27 | 2007-10-04 | Hideki Yamamoto | Method for recovering mixed acid with increased compositional ratio of hydrofluoric acid from waste mixed acid liquid containing hydrofluoric acid |
| US20080053815A1 (en) * | 2006-08-31 | 2008-03-06 | Wacker Chemie Ag | Method for processing an etching mixture which is formed during the production of highly pure silicon |
| CN103086555A (en) * | 2011-10-31 | 2013-05-08 | 库特勒自动化***(苏州)有限公司 | Treatment system and treatment method for silicon wafer etching waste water |
| JP2013163168A (en) * | 2012-02-13 | 2013-08-22 | Kurita Water Ind Ltd | Apparatus and method for refining fluoro-nitric acid waste solution |
| CN102745837A (en) * | 2012-07-18 | 2012-10-24 | 上海交通大学 | Method for treating and recycling glass thinning and etching waste liquor |
| CN103213991A (en) * | 2013-04-28 | 2013-07-24 | 苏州晶瑞化学有限公司 | Recovery and cyclic utilization technology for electronic-level waste acid mixture |
| CN104986771A (en) * | 2015-07-02 | 2015-10-21 | 苏州晶洲装备科技有限公司 | Treatment method for multi-crystalline silicon texturization etching waste liquid |
| CN204981156U (en) * | 2015-07-02 | 2016-01-20 | 苏州晶洲装备科技有限公司 | Recovery system of recycling of polycrystalline silicon making herbs into wool sculpture waste liquid |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640349A (en) * | 2018-05-25 | 2018-10-12 | 南京八度阳光太阳能科技有限公司 | A kind of silicon solar cell making herbs into wool waste collecting device |
| CN108716020A (en) * | 2018-05-29 | 2018-10-30 | 南京八度阳光太阳能科技有限公司 | A kind of making herbs into wool waste material recycling device used for solar batteries |
| CN110844885A (en) * | 2019-09-06 | 2020-02-28 | 浙江东氟塑料科技有限公司 | Method for recovering and regenerating hydrofluoric acid from waste liquid |
| CN111573640A (en) * | 2020-04-29 | 2020-08-25 | 南京理工大学 | Method and system for producing high-purity nitric acid by recovering fluorine-containing dilute nitric acid waste liquid |
| CN111573640B (en) * | 2020-04-29 | 2022-11-25 | 南京理工大学 | Method and system for producing high-purity nitric acid by recycling fluorine-containing dilute nitric acid waste liquid |
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Application publication date: 20170901 |
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